SPM cantilever and fabricating method thereof

ABSTRACT

Disclosed herein is SPM cantilever having a support portion, a lever portion extended from the support portion and a probe portion formed at a free end of the lever portion, said probe portion having a generally plate-like form and the probe portion having an additionally sharpened terminal end portion. The terminal end portion has its length greater than the plate thickness thereof and is reduced in thickness toward a tip of the terminal end portion, and the tip is located inwardly of the planes extended from the front and back sides of a base portion of the plate-like probe portion.

This application claims benefit of Japanese Application No. 2002-313599filed in Japan on Oct. 29, 2002, and is a division of U.S. patentapplication Ser. No. 10/694,358, filed on Oct. 28, 2003, the contents ofwhich are incorporated by this reference.

BACKGROUND OF THE INVENTION

The present invention relates to SPM cantilevers and fabricating methodsthereof for use in Scanning Probe Microscopies (SPM) such as AtomicForce Microscopy (AFM). Scanning Probe Microscopies (SPM), apparatushaving an atomic-order measuring resolution such as for use in measuringsurface irregularities, are now widely used. In recent years, however,measurements at yet higher resolutions are demanded. For this reason, itis desirable for the cantilever used in SPM to be provided with a probeportion sharpened at its terminal end and at the same time having highaspect ratio.

Among such SPM cantilevers is a cantilever as disclosed in JapanesePatent No. 2624873. The SPM cantilever uses a silicon oxide film as thelever material. In particular, a resist film is formed on the surface ofa thermally oxidized silicon film having a thickness of 1 to 2 μm and asharpened portion is formed in the resist film by using photoetchingtechnologies. A silicon oxide film probe portion having a smaller radiusof curvature than the sharpened portion formed of the resist film isthen formed by effecting an isotropic etching by a buffer etchingsolution. With such fabricating method of SPM cantilever, an SPM probeportion can be formed as having a radius of curvature of 0.1 μm or lessat its terminal end by using the conventional photoetching technologiesand also as having favorable adhesion between a cantilever supportportion and the lever by using the thermally oxidized silicon as thelever material.

Further, a processing method of cantilever using focused ion beam (FIB)has been disclosed in Japanese Patent No. 2984094. In the processingmethod, a focused ion beam is caused to irradiate a probe's terminal endportion with arbitrarily changing the scanning direction so as toprocess the probe terminal end portion into a sharpened form. With suchprocessing method of cantilever, it is possible to arbitrarily changethe vertical angle at a terminal end of the probe and to vary an aspectratio thereof. At the same time the radius of curvature of the terminalend of the probe can be processed into 50 nm or less.

The previously suggested cantilevers as described above, however, haveproblems as follows. First, a problem in the cantilever disclosed inJapanese Patent No. 2624873is that it becomes impossible to accuratelyascertain the surface irregularities of a sample,-even though theterminal end of the probe can be sharpened. This problem will bedescribed below with reference to FIG. 1. FIG. 1 shows the relationbetween the probe's terminal end and a sample to be measured, including:a lever portion 101; a plate-like probe portion 102 of silicon oxidefilm formed on a free end of the lever portion; and a sample 103 to bemeasured. Supposing as shown in FIG. 1, L₁ as the plate thickness of theprobe portion and L₂ as the length of the sharpened terminal end portionformed by etching in the case where an isotropic wet etching of theplate-like silicon oxide film probe portion 102 is effected by using aresist mask, L₁ and L₂ are equal to each other in length or, morelikely, the relationship of L₁>L₂ holds due to the fact that theterminal end portion is etched away also from sides of the resist mask.Accordingly, length L₂ of the probe terminal end portion to be sharpenedbecomes shorter. If this is used in measuring the sample 103 which hasrelatively large irregularities, those portions other than the probe'sterminal end are brought into contact with the irregularities of thesample 103 to be measured so that it becomes impossible to accuratelyascertain configuration of the irregularities.

Also, since the silicon oxide is etched away in a short time period byfluoric acid, the fabrication of a sharpened probe portion of the orderof nanometers with controlling variance thereof is difficult due to thevariance in etching if a plurality of cantilevers each having probeportion are to be fabricated within a wafer.

Of the cantilever disclosed in Japanese Patent No. 2984094, on the otherhand, though the forming of a probe portion having high aspect ratio ispossible, the radius of curvature of the terminal end of the probeportion is difficult to be regulated to result a lower yield, since FIBprocessing must be performed for each one cantilever. Also, in the caseof a thin lever portion, warping of the lever might be caused due todamage or heat in the FIB processing. Further, in addition to theexpensiveness of FIB apparatus, there is a problem of increased cost forexample because of the excessively long time to be consumed in formingseveral hundred cantilevers on a wafer.

SUMMARY OF THE INVENTION

It is an object of the present invention to provide a cantilever havinga silicon nitride probe portion and simple fabricating method thereof inwhich a terminal end of the probe portion is sharpened in a wellregulated manner and which is capable of adopting a high aspect ratio,processed at high yield and also capable of reducing costs. It isanother object of the invention to provide a fabricating method ofcantilever in which a cantilever having a sharpened probe portion can bereadily fabricated without depending on the surface irregularities of asubstrate as far as the substrate is capable of being covered by asilicon nitride film. It is a further object of the invention to providea fabricating method of cantilever in which a terminal end of probe canbe sharpened even if a very thin lever material is used.

In a first aspect of the invention, there is provided SPM cantileverhaving a support portion, a lever portion extended from the supportportion and a probe portion formed at a free end of the lever portion.The probe portion has a generally plate-like form and the probe portionhas an additionally sharpened terminal end portion. The terminal endportion has its length greater than the plate thickness thereof and isreduced in thickness toward a tip of the terminal end portion. The tipis located inwardly of the planes extended from the front and back sidesof a base portion of the plate-like probe portion.

The SPM cantilever according to the first aspect may employ aconstruction where the probe portion is generally triangular and twosides containing the terminal end portion are inwardly bent.

In a second aspect of the invention, there is provided SPM cantileverhaving a support portion, a lever portion extended from the supportportion and a probe portion formed at a free end of the lever portion.The probe portion is generally pyramidal or conic and the pyramidal orconic probe portion has an additionally sharpened terminal end portion.

The SPM cantilever according to the second aspect may employ aconstruction where the probe portion is generally in the form of atriangular pyramid or in the form of a circular cone.

The SPM cantilever according to the first or second aspect may employ aconstruction where the probe portion is formed of silicon nitride.

In a third aspect of the invention, there is provided a fabricatingmethod of SPM cantilever having a support portion, a lever portionextended from the support portion, and a probe portion formed at a freeend of the lever portion, including the steps of: depositing a siliconnitride film to become the probe portion and the lever portion on asilicon substrate derived from silicon wafer; patterning the siliconnitride film deposited on the silicon substrate into a configurationhaving an acute angle portion for forming the probe portion; forming aprotecting film with exposing the acute angle portion of the patternedsilicon nitride film; effecting a low-temperature thermal oxidation ofthe exposed acute angle portion of the silicon nitride film; and forminga sharpened probe portion by removing by means of fluoric acid theoxidized portion on the surface of the acute angle portion of thesilicon nitride film treated of the low-temperature thermal oxidation.

In a fourth aspect of the invention, there is provided a fabricatingmethod of SPM cantilever having a support portion, a lever portionextended from the support portion, and a probe portion formed at a freeend of the lever portion, including the steps of: forming a siliconprojection for forming the probe portion on a silicon substrate derivedfrom silicon wafer; depositing a silicon nitride film to become theprobe portion and the lever portion on the silicon substrate having thesilicon projection formed thereon; effecting a low-temperature thermaloxidation of the silicon nitride film formed on the projection of thesilicon substrate; and forming a sharpened probe portion by removing bymeans of fluoric acid the oxidized portion on the surface of the siliconnitride film treated of the low-temperature thermal oxidation.

The silicon nitride film in the fabricating method of SPM cantileveraccording to the third or fourth aspect preferably has a silicon contentin terms of an elemental ratio between silicon and nitrogen greater than3:4.

The silicon nitride film in the fabricating method of SPM cantileveraccording to the third or fourth aspect is preferably formed by chemicalvapor deposition.

The low-temperature thermal oxidation in the fabricating method of SPMcantilever according to the third or fourth aspect is effectedpreferably at oxidizing temperatures above 900° C. and below 1050° C.

The low-temperature thermal oxidation on the silicon nitride film in thefabricating method of SPM cantilever according to the third or fourthaspect is preferably effected so that an oxide film having a filmthickness of 50 nm or more be formed on (100) silicon lattice plane ofthe silicon substrate adjacent thereto.

In a fifth aspect of the invention, there is provided SPM cantileverfabricated by a fabricating method of cantilever having a supportportion, a lever portion extended from the support portion, and a probeportion formed at a free end of the lever portion, including the stepsof: depositing a silicon nitride film to become the probe portion andthe lever portion on a silicon substrate derived from silicon wafer;patterning the silicon nitride film deposited on the silicon substrateinto a configuration having an acute angle portion for forming the probeportion; forming a protecting film with exposing the acute angle portionof the patterned silicon nitride film; effecting a low-temperaturethermal oxidation of the exposed acute angle portion of the siliconnitride film; and forming a sharpened probe portion by removing by meansof fluoric acid the oxidized portion on the surface of the acute angleportion of the silicon nitride film treated of the low-temperaturethermal oxidation.

The SPM cantilever according to the fifth aspect may employ aconstruction where the probe portion is generally triangular and twosides containing a terminal end portion thereof are inwardly bent.

In a sixth aspect of the invention, there is provided SPM cantileverfabricated by a fabricating method of cantilever having a supportportion, a lever portion extended from the support portion, and a probeportion formed at a free end of the lever portion, including the stepsof: forming a silicon projection for forming the probe portion on asilicon substrate derived from silicon wafer; depositing a siliconnitride film to become the probe portion and the lever portion on thesilicon substrate having the silicon projection formed thereon;effecting a low-temperature thermal oxidation of the silicon nitridefilm formed on the projection of the silicon substrate; and forming asharpened probe portion by removing by means of fluoric acid theoxidized portion on the surface of the silicon nitride film treated ofthe low-temperature thermal oxidation.

The SPM cantilever according to the sixth aspect may employ aconstruction where the probe portion is generally pyramidal or conic.

The SPM cantilever according to the sixth aspect may employ aconstruction where the probe portion is generally in the form of atriangular pyramid or in the form of a circular cone.

The silicon nitride film in the SPM cantilever according to the fifth orsixth aspect preferably has a silicon content in terms of an elementalratio between silicon and nitrogen greater than 3:4.

The silicon nitride film in the SPM cantilever according to the fifth orsixth aspect is preferably formed by chemical vapor deposition.

The low-temperature thermal oxidation in the SPM cantilever according tothe fifth or sixth aspect is effected preferably at oxidizingtemperatures above 900° C. and below 1050° C.

The low-temperature thermal oxidation on the silicon nitride film in theSPM cantilever according to the fifth or sixth aspect is preferablyeffected so that an oxide film having a film thickness of 50 nm or morebe formed on (100) silicon lattice plane of the silicon substrateadjacent thereto.

BRIEF DESCRIPTION OF THE DRAWINGS

FIG. 1 typically shows the relation between the probe's terminal end ofthe conventional SPM cantilever and a sample to be measured.

FIG. 2 is a partially omitted perspective view showing construction of afirst embodiment of SPM cantilever according to the invention.

FIGS. 3A, 3B and 3C show the form of the probe portion of the cantileveraccording to the first embodiment as seen from the three directions ofA, B, C shown in FIG. 2.

FIGS. 4A to 4I illustrate the fabricating steps for explaining thefabricating method of the cantilever according to the first embodimentshown in FIG. 2.

FIGS. 5A and 5B are enlarged views of the step shown in FIG. 4F in thefabricating steps of the cantilever according to the first embodiment.

FIG. 6 is an enlarged view typically showing the relation between theprobe's terminal end of the cantilever according to the first embodimentof the invention shown in FIG. 2 and a sample to be measured.

FIG. 7 is a perspective view showing construction of the probe portionof the cantilever according to a second embodiment of the invention.

FIGS. 8A to 8K illustrate the fabricating steps for explaining thefabricating method of the cantilever according to the second embodimentshown in FIG. 7.

FIGS. 9A and 9B illustrate in detail the step shown in FIG. 8D in thefabricating steps of the cantilever according to the second embodiment.

DESCRIPTION OF THE PREFERRED EMBODIMENTS

A first embodiment of the invention will now be described. An overallconstruction of the lever portion and probe portion of the firstembodiment of SPM cantilever according to the invention is shown in FIG.2, and the configurations as seen from the directions of A to C in FIG.2 of the probe portion are shown in FIGS. 3A, 3B and 3C, respectively.As shown in these figures, a probe portion 2 is formed toward the freeend of a lever portion 1. Here the probe portion 2 is constituted by aplate-like thin film formed toward the free end of the lever portion 1,and an acutely angled terminal end portion 3 of the probe portion 2 islocated at the free end of the lever.

The probe portion 2 is inclined by an angle of 54.7 degreescorresponding to the lattice plane (111) of silicon with respect to thelever portion 1 at its boundary 4 to the lever portion 1. Further, twosides 2 a, 2 b of the probe portion 2 that contain the terminal endportion 3 are bent toward the inner side. In other words, it is formedinto such a shape that, of the portions having the same width as thelever portion 1, those portions unnecessary as the probe portion 2 arecut off. By such construction, the weight of the probe portion 2 isreduced so that a drop in resonance frequency can be prevented. At thesame time, an aspect ratio of the configuration of the terminal endportion 3 of the probe portion 2 is improved so that a sample ofnarrower measurement intervals can be measured. Further, a damping incantilever oscillation due to the air or water surrounding thecantilever can be reduced. The terminal end portion 3 of the probeportion 2 has a radius of curvature of 20 nm or less and is very slenderas having its length exceeding the plate thickness (film thickness), i.e., the probe structure has a probe terminal end portion of high aspectratio.

The SPM cantilever having such construction makes it possible to achievean SPM cantilever having a probe portion of the structure by which asufficient measurement down to a bottom surface of concave is possibleeven if the sample has surface irregularities of relatively large aspectratio. Also, since the terminal end of the probe portion can be broughtinto contact substantially vertically with the sample to be measured,measurements at high resolution become possible.

The fabricating method of SPM cantilever according to the firstembodiment having the above described construction will now be describedby way of the fabricating steps shown in FIGS. 4A to 4I. First, asilicon wafer of lattice plane (100) having Orientation Flat in<011>direction is prepared and used as a substrate 11. As shown in FIG.4A, then, a mask 12 for the cantilever support portion is formed on theback side of the silicon substrate 11. Here a silicon oxide film forexample is suitably used as the mask 12. A mask 13 for forming the probeportion is formed by a silicon nitride film at a predetermined location.At the same time, a silicon nitride film 14 for protecting thecantilever support portion mask 12 is formed on the back side of thesilicon substrate 11.

The silicon front side having the probe portion forming mask 13 thereonis then subjected to anisotropic wet etching by means of an alkaliaqueous solution such as KOH (potassium hydroxide) or TMAH (tetramethylammonium hydroxide) to form a step difference 15 for forming the probeportion as shown in FIG. 4B on one side of the silicon substrate 11. Theprobe portion forming mask 13 and the back-side silicon nitride film 14are then removed for example by heat phosphoric acid.

As shown in FIG. 4C, then, a silicon nitride film 16 to become the leverportion and probe portion is formed together with a back-side siliconnitride film 16′. Here the silicon nitride film 16, a silicon nitridefilm containing more silicon than a normally used silicon nitride film(Si₃N₄), is deposited by Low Pressure Chemical Vapor Deposition(LP-CVD).

In particular, this can be achieved by increasing the ratio ofdichlorosilane to a level higher than normal in the flow ofdichlorosilane and ammonia at the time of deposition. While the filmthickness of silicon nitride is variable according to the desiredcharacteristics, it in this case is 0.1 μm, rather thinner than anormally used silicon nitride cantilever film thickness of 0.4 μm, inanticipation of a cantilever having a resonance frequency of 1 MHz andspring constant of 0.1 N/m. Naturally, however, the film thickness ofsilicon nitride is not limited to such a value.

By as described using a silicon nitride film having a higher siliconcontent, in particular the silicon nitride film containing more siliconthan an elemental ratio of 3:4 between silicon and nitrogen, warping atthe lever portion or crack at the terminal end of the probe portion canbe prevented. Further, the reaction of silicon atoms within the siliconnitride film and oxygen atoms is accelerated during the oxidation,resulting in an advantage of promoting the sharpening effect.Furthermore, use of CVD method in forming the silicon nitride film makesit possible to adjust the elemental ratio between silicon and nitrogenwithin the silicon nitride film so that a fine film having less internalstress be formed. Also, since the silicon nitride film can be formed ona substrate of various shapes or materials, the scope of its applicationcan be widened.

Next, as shown in FIG. 4D, the silicon nitride film 16 is patterned byphotolithography and an etching of the silicon nitride film 16 is theneffected for example by RIE (Reactive Ion Etching) to form a probeportion 17 and lever portion 18 of the pattern as previously shown inFIG. 2. At this time, the tip of the terminal end portion of the probeportion 17 suffices to have a small radius of curvature within apossible range. If, for example, the radius of curvature is of the orderof 100 nm, a sufficiently small radius of curvature can be obtained inthe succeeding steps as will be described later.

Subsequently, as shown in FIG. 4E, after depositing a silicon oxide filmall over by CVD method to a thickness of about 0.5 μm, the silicon oxidefilm over the silicon substrate 11 at the probe portion 17 and avicinity thereof is removed with preserving only the portion over thelever portion 18 as a protecting film 19.

Next, the sharpening of the terminal end portion of the probe portion iseffected. As shown in FIG. 4F, a low-temperature thermal oxidationtreatment is effected to form a silicon oxide film 20 only over thesilicon substrate 11 at the terminal end portion of the probe portion 17and a vicinity thereof where the protecting film 19 is absent. It shouldbe noted that the dotted line in FIG. 4F indicates the position of anupper surface of the silicon substrate 11 before the low-temperaturethermal oxidation treatment. Here the low-temperature thermal oxidationtreatment is effected in a steam atmosphere. To obtain a sharpeningeffect of the terminal end portion of the probe portion, thelow-temperature thermal oxidation treatment is preferably effected attemperatures above 900° C. and below 1050° C. to an extent where thefilm thickness of the silicon oxide film formed on the silicon substratesurface in the vicinity of the probe portion 17 becomes 50 nm or more.

The reason for setting the temperature of the thermal oxidationtreatment in this manner is that oxidation is caused to unevenly proceedfrom the front and back sides as well as from lateral faces of thesilicon nitride film by lowering the oxidizing temperature so that asharpened part can be formed on the silicon nitride film of the portionnot oxidized. In other words, the silicon nitride film thickness at theterminal end portion of the probe portion becomes thinner so that aprobe portion made of silicon nitride having a sharpened tip can beformed. It should be noted that a problem of longer treatment time dueto lowered oxidation treatment rate occurs if the temperature of thelow-temperature thermal oxidation treatment is lower than 900° C.Further, if it is set above 1050° C., the silicon nitride film, which issusceptible to thermal stress, is affected by thermal stress so that aproblem of crack or the like is caused.

Further, the reason for defining the film thickness of the silicon oxidefilm to be formed on the vicinity silicon substrate surface as describedabove is as follows. If the thickness of the oxide film on the vicinitysilicon substrate surface is thinner than 50 nm, the oxide film to beformed on the silicon nitride film also becomes thinner, i. e., onlyseveral nanometers so that a sufficient sharpening effect of theterminal end portion of the probe portion is difficult to be obtained.Accordingly, the film thickness of the silicon nitride at the terminalend portion of the probe portion 17 is reduced so as to make its tipsharpened by a low-temperature thermal oxidation treatment under theabove described conditions, whereby the probe portion 17 can be obtainedas having its terminal end portion sharpened in a relatively longerextent.

The manner of the terminal end portion of the probe portion 17 at thetime of such low-temperature thermal oxidation treatment is shown in anenlarged manner in FIG. 5A. In particular, when a low-temperaturethermal oxidation treatment is performed to oxidize the silicon nitridefilm 16 for forming the probe portion 17, oxidation is advanced not onlyfrom the front side of the silicon nitride film 16 which will become theterminal end portion of the probe portion 17 but also from the back sideand two lateral faces of the silicon nitride film 16 which will becomethe terminal end portion of the probe portion 17. Accordingly, theplate-like silicon nitride film 16 is oxidized from the front and backsides and also from the two lateral faces thereof so that the siliconoxide film 20 be formed. A high aspect ratio is thereby achieved of theterminal end portion of the probe portion 17 where the sharpening ismore intense toward its tip.

Next, the silicon oxide film 20 is removed by fluoric acid to form theprobe portion 17 having a radius of curvature of 20 nm or less as shownin FIG. 5B. Here, since the silicon nitride film 16 of the portion tobecome the lever portion 18 is covered by the protecting film 19 of thesilicon oxide film deposited by CVD method, the silicon nitride film 16to become the lever portion 18 is not oxidized even by thelow-temperature thermal oxidation treatment and thus is not reduced infilm volume by the fluoric acid treatment. The flatness of the leverportion is also kept.

Subsequently to the step shown in FIG. 4F as described, the siliconnitride film 16′ on the back side of the silicon substrate 11, which hasbeen protecting the support portion, is then removed so as to expose thesupport portion mask 12 on the surface, while preserving the protectingfilm 19 of silicon oxide film and the silicon oxide film 20 due to thelow-temperature thermal oxidation treatment as shown in FIG. 4G. Asilicon substrate front side protecting film 21 is then formed forexample by CVD method to a thickness of about 1 μm.

Next, as shown in FIG. 4H, an alkaline etchant for example typicallyrepresented by KOH is used to perform anisotropic etching from the sideopposite to the projecting direction of the probe portion 17 to form asupport portion 22 for holding the cantilever. Thereafter, theprotecting film 19, silicon oxide film 20 and front side protecting film21 are removed.

Finally, as shown in FIG. 4I, a reflecting film 23, if required, isformed on the lever portion 18 on the side opposite to the directiontoward which the probe portion 17 is caused to project so that acantilever 24 having the plate-like probe portion 17 is complete. Thereflecting film 23 is formed for example by evaporating gold. Thereflecting film, though formed in this case, is not necessarilyrequired, and, in some cases, it is not necessary to form a reflectingfilm.

A further explanation will be made below with respect to the reason whysilicon nitride having greater silicon content is used as the siliconnitride film for constructing the probe portion and lever portion of SPMcantilever according to the first embodiment. In particular, the reasonis that the reaction between silicon atoms in the silicon nitride filmand oxygen atoms in the oxygen atmosphere is accelerated during thesharpening step so that an advantage of promoting the surface oxidationresults. Specifically, while an elemental ratio between silicon (Si) andnitrogen (N) of the silicon nitride film in the range of 0.75<Si/N≦1.3is used in the present embodiment, such range is an optimal elementalratio range for the structure of a thin film such as cantilever.Particularly regarding stress, if the elemental ratio is Si/N≦0.75, anintense tensile stress of 1,000 MPa or above results. Because of this,warping at the lever portion occurs or the tip of the probe portion iscracked due to stress.

In the range of Si/N>1.3, on the other hand, since Si ispolycrystallized and causes a precipitation, the surface coarseness isworsened and it becomes disadvantageous for example for a cantilever inwhich a smooth lever portion surface or probe portion surface isdesired. Also in a subsequent silicon etching process, an etchant maypermeate from the polycrystallized silicon portion to result an abnormaletching. To prevent such abnormal etching, the above described elementalratio range is used.

By such fabricating method, the cantilever made of silicon nitridehaving a radius of curvature at the tip of the probe portion sharpenedto 20 nm or less and at the same time having a high aspect ratio thereofcan be readily fabricated without using a high precision apparatus whichis expensive. Further, since the probe portion having the sharpenedterminal end portion can be fabricated in a well regulated manner and athigh yield, costs can also be reduced. Furthermore, batch fabricationand processing of a plurality of cantilevers at wafer level becomepossible.

In particular, unlike the conventional method in which a resist mask isprepared and an underetching is effected while regulating the etchantand time, the length of the sharpened portion of the probe terminal endportion in the fabricating method according to the present embodiment isnot restricted by the limitation due to the permeation of etchant underthe mask so that the sharpened portion (terminal end portion) havinggreater length can be made. Further, in the fabricating method accordingto the present embodiment, it is adequate that only the oxidized portionformed on the silicon nitride film surface be entirely etched away byfluoric acid. It is thereby also possible to secure far greaterprocessing margin for example in control of the temperature andconcentration of etchant and control of etching time as compared to anisotropic wet etching of which control is generally considered to bedifficult.

In the case where a further improvement in the aspect ratio of the probeportion or further sharpening of the tip of the terminal end portion isdesired, the above described process, i.e., the forming of an oxide filmby low-temperature thermal oxidation treatment and the removing of theoxide film by fluoric acid can be repeated for a plurality of times toadditionally promote the sharpening. In particular, while a long time isrequired to form an oxide film of desired film thickness on the siliconnitride film by one time of low-temperature thermal oxidation treatment,a similar result as the forming of the oxide film of the desired filmthickness can be obtained in a shorter time period by repeating aplurality of times the forming processing of an oxide film having a filmthickness thinner than the desired film thickness. Also, the sharpeningof the probe portion can be additionally promoted by previously formingan optimal acute angle pattern of silicon nitride film.

Further, the probe portion of the cantilever fabricated as described isin the form of a plate. The terminal end portion 3 of the probe portion2(17) is located as shown in FIG. 6 inwardly of the imaginary extendedplanes (indicated by dotted lines) of the two sides of the base portionof the plate-like probe portion 2 so that the tip of the terminal endportion 3 is extended toward the inside of the front and back sides ofthe plate-like probe portion 2. It is thereby possible for the tip ofthe probe portion 2 at the time of measuring to contact a sample 5 at anear-perpendicular angle so that the resolution is not likely to belowered.

The inwardly curved configuration of the terminal end portion 3 of thesharpened probe portion 2 is different from the conventional case asshown in FIG. 1 that depends on isotropic wet etching. In particular,supposing L₁ as the plate thickness of the probe portion 2 and L₂ as thelength of the sharpened terminal end portion 3 of the probe portion 2,the relation of L₁≧L₂ holds in the conventional cantilever. In thecantilever of the invention, on the other hand, the relation is L₁<L₂and results in a configuration where the aspect ratio of the sharpenedprobe terminal end portion 3 is greater. In particular, the length L₂ ofthe sharpened portion (terminal end portion 3) is longer than thethickness L₁ of the plate-like probe portion 2. A measurement even onthe surface irregularities of the sample 5 thereby becomes possiblewithout causing a portion other than the tip of the probe portion tocontact thereat.

Further, of the cantilever according to the present embodiment, theprobe portion is located on the free end of the lever portion. Thepositioning at the time of measuring (scanning) of the probe portion toa location to be observed on the sample can thus be easily effected in ashort time by attaching it to SPM apparatus into which an opticalmicroscope is combined. Further, the sample to be measured and the tipof the probe portion can be brought into contact substantiallyvertically with each other so that a high-resolution measurement becomespossible.

It should be noted that the fabricating method of SPM cantileveraccording to the present embodiment has been shown as that using RIE inetching the silicon nitride film in the step shown in FIG. 4D. It ishowever not limited to the use of RIE and other dry etchers such asICP-RIE or an wet etching for example of hot phosphoric acid can also beused. This is because the surface oxidation is not affected by theconfiguration of the silicon nitride film before the oxidation step.

Further, since the fabricating method of cantilever explained in thepresent embodiment is characterized in the sharpening process of theprobe portion, it can be applied also to the fabrication of cantileversof other forms as far as the probe portion is fundamentally made ofsilicon nitride. For example, even in a cantilever where the probeportion is formed of silicon nitride and the lever portion is made of asingle crystal silicon, it is possible to cover the single crystalsilicon portion with a protecting mask so as to sharpen-only the siliconnitride probe portion by the technique according to the presentembodiment. In such cantilever having a lever portion formed of singlecrystal silicon, a greater lever thickness can be readily achieved sothat it is advantageous in those SPM cantilevers of which relativelygreater spring constant and higher resonance frequency are required.

In a summary of the fabricating method according to the above firstembodiment, since uniform probe portions can be formed all over a waferby combining the simple processes, i.e., low-temperature thermaloxidation treatment and wet etching process by fluoric acid, it ispossible to readily fabricate a cantilever having a generally plate-likeprobe portion of which the terminal end portion can be sharpened in awell regulated manner and which has a high aspect ratio. Further, sincethe probe portions of a large number of cantilevers to be formed on aplurality of pieces of wafers can be subjected to the sharpeningtreatment at once, the yield thereof is high and costs can be reduced.Further, since only the terminal end of the probe portion is oxidized,the oxidation does not-affect the lever portion and other parts at all.

A second embodiment of the invention will now be described. While thedescription in the first embodiment has been made with respect to theplate-like probe portion, this embodiment will be described with respectto the probe portion in a pyramidal or conic form, specifically of atriangular pyramid. The structure of the probe portion of cantilever foruse in scanning probe microscopy (SPM) according to this embodiment isshown in FIG. 7. Referring to FIG. 7, a probe portion 32 is formedtoward the free end of a lever portion 31 extended from a supportportion (not shown). Here the probe portion 32 has a triangularpyramidal structure, and a tip 33 of the probe portion is slenderlysharpened by sharpening treatment and points the direction of the freeend of the lever portion 31. It should be noted that the radius ofcurvature of the probe portion tip is extremely sharpened to be 20 nm orless and the probe portion has a high aspect ratio.

By thus forming the probe portion into a pyramidal or conic form, theprobe portion is provided with a high mechanical rigidity so that themechanical characteristics of SPM cantilever can be stabilized and thestrength of the probe portion can be increased. The cantilever isachieved as having the probe portion which is additionally sharpened atthe terminal end portion thereof and has a length required for measuringrelatively large surface irregularities of a sample. Further, by formingthe probe portion into a triangular pyramidal form, it can be readilyfabricated and steady measurements become possible. It is also possibleto form the probe portion into a circular cone. In such case, steadymeasurements become possible due to the fact that the terminal endportion of the probe portion becomes symmetrical.

The fabricating steps of cantilever according to the second embodimentwill now be described by way of FIGS. 8A to 8K. First, a silicon waferof lattice plane (100) having Orientation Flat in <011> direction isprepared and used as a substrate 41. Next, as shown in FIG. 8A, a mask42 for forming the support portion is formed by a silicon oxide film ata predetermined location on the back side of the silicon substrate 41.

Next, a mask 43 for forming a convex portion is formed on the siliconsubstrate 41 and, as shown in FIG. 8B, a vertical etching of the siliconsubstrate front side is effected to a depth of the order of the probelength by Deep-RIE (Reactive Ion Etching) to form a convex portion 44for forming the probe portion. Here a silicon nitride film is suitablyused as the convex portion forming mask 43. Further, at the time offorming the mask 43 of silicon nitride film, a protecting film 45 ofsilicon nitride film is also formed on the back side of the siliconsubstrate 41.

Next, after effecting thermal oxidation with preserving the mask 43 toform a silicon oxide film 46 over the entire surface, the siliconnitride film 43 on the convex portion 44 and the silicon oxide film 46formed on the silicon nitride film 43 are removed as shown in FIG. 8C. Aheat phosphoric acid for example is suitably used for the removal of thesilicon nitride film 43.

Next, as shown in FIG. 8D, the convex portion 44 having an exposedsilicon substrate surface thereon is subjected to anisotropic wetetching for example by potassium hydroxide (KOH) solution. Thedifference in etching rates of lattice plane orientation of silicon isthen used to form a silicon surface projection 47 in a triangularpyramidal form constructed by lattice plane (111).

Here the depth of etching suffices to be of the same level as the probelength.

The processing step of forming the triangular pyramidal silicon surfaceprojection 47 will now be described in further detail by way of FIGS. 9Aand 9B. FIG. 9A is an enlargement of FIG. 8D and is a sectional viewalong line X-X′ of the top view shown in FIG. 9B. The convex portionforming mask 43 shown in FIG. 8B is rhombus-shaped so that the probeportion forming convex portion 44 shown in FIG. 8C is formed in arhombus. Accordingly, if the silicon oxide film 46 formed on thesubstrate front side and the lateral faces of the rhombus convex portionas shown in FIG. 8C is used as the mask to effect an anisotropic wetetching of the convex portion 44, triangular pyramidal silicon surfaceprojections 47 are formed on the four corners of the rhombus convexportion 44 as shown in FIGS. 9A and 9B. It should be noted that, in FIG.9B, the dotted line indicates the configuration of the patterning ofcantilever to be performed in a subsequent step.

Next, as shown in FIG. 8E, after etching the silicon oxide film 46formed on the front side of the silicon substrate 11 for example byfluoric acid and also removing the protecting film 45 of silicon nitridefilm formed on the back side of the silicon substrate 11 by heatphosphoric acid, a silicon nitride film 48 having a greater siliconcontent than a normal silicon nitride film to become the lever portionand probe portion is deposited by LP-CVD. In particular, this can beachieved by increasing the ratio of dichlorosilane in the flow ratio ofdichlorosilane and ammonia at the time of deposition. Here the tip ofthe silicon nitride film 48 to become the probe portion has a radius ofcurvature of about 50 nm. At the same time, a silicon nitride filmsimilar to the silicon nitride film 48 deposited on the back side of thesilicon substrate is used again as a protecting film 45′ of the supportportion forming mask pattern 42 on the back side of the wafer.

Next, as shown in FIG. 8F, the deposited silicon nitride film 48 ispatterned into the shape of a cantilever by photolithography and thesilicon nitride film 48 is etched for example by RIE (Reactive IonEtching) to form a probe portion 49 and lever portion 50. It should benoted that a projection 49′ of an identical configuration as the probeportion 49 is also formed at the same time.

Subsequently, as shown in FIG. 8G, after depositing a silicon oxide filmto a thickness of about 0.5 μm by CVD method, the silicon oxide filmover the terminal end portion of the probe portion 49 and on the siliconsubstrate 41 in a vicinity thereof is removed while preserving it onlyover the lever portion 50 containing the projection 49′ as a protectingfilm 51.

Next, the sharpening of the probe portion 49 is effected. As shown inFIG. 8H, a low-temperature thermal oxidation treatment is first effectedto form an oxide film 52 only over the probe portion 49 and on thesilicon substrate surface in a vicinity thereof other than the regionwhere the protecting film 51 is formed. Here the low-temperature thermaloxidation treatment is effected in a steam atmosphere; and, in order toobtain a sharpening effect, the treatment is preferably of such a levelthat the film thickness of the oxide film on the silicon substratesurface becomes 50 nm or more under the temperatures above 900° C. andbelow 1050° C.

The reason for setting the temperature of the thermal oxidationtreatment in this manner is that oxidation is caused to unevenly proceedfrom the silicon nitride film surface of the probe portion 49 bylowering the oxidizing temperature so that a sharpened part can beformed on the silicon nitride film of the portion not oxidized. Further,the reason for defining the film thickness of the oxide film on thesilicon substrate surface as described is that, if the film thicknessthereof is too thin, an adequate sharpening effect of the probe portion49 formed of silicon nitride film is difficult to be obtained. By suchlow-temperature thermal oxidation treatment, the silicon nitride at theterminal end portion of the probe portion 49 is reduced in its filmthickness and sharpened in a similar manner as the first embodiment.

In particular, when the low-temperature thermal oxidation treatment iseffected to oxidize the silicon nitride film for forming the probeportion 49, the surface of the silicon nitride film at the probeterminal end portion is oxidized from the surrounding of the triangularpyramidal silicon nitride film so as to form an oxide film. A highaspect ratio of the probe portion 49 is thereby achieved such that thesharpening is more intense toward the tip thereof. Accordingly, byremoving the oxide film 52 by fluoric acid at a subsequent step, a probeportion having a radius of curvature of 20 nm or less is formed. Here,since the silicon nitride film of the portion becoming the lever portion50 is covered by the protecting film 51 deposited by CVD method, thesilicon nitride film constituting the lever portion 50 is not oxidizedeven by the low-temperature thermal oxidation treatment and thus is notreduced in film volume by the fluoric acid treatment. Further, theflatness of the lever portion is also kept.

Subsequently to the processing step shown in FIG. 8H as described, asilicon oxide film 53 by CVD method is then formed as shown in FIG. 8Ias a protecting film of cantilever all over the front side of thesilicon substrate. Next, as shown in FIG. 8J, the protecting film 45′ onthe back side of the silicon substrate is removed and an alkali etchanttypically represented for example by KOH is used to effect anisotropicetching from the side opposite to the projecting direction of the probeportion 49 to form a support portion 54 for holding the cantilever.

Finally, as shown in FIG. 8K, the silicon oxide film 53 by CVD methodformed all over the front side of the silicon wafer as the protectingfilm of the cantilever, the protecting film 51 of the silicon oxidefilm, and the oxide film 52 by low-temperature thermal oxidationtreatment, as well as the support portion forming mask 42 are etchedaway by fluoric acid to complete a cantilever 55 having the triangularpyramidal probe portion 49. Here, while the projection 49′ of theconfiguration similar to the probe portion 49 is also formed in additionto the probe portion, this causes no problem if the original maskpattern is formed so that it be formed at a position other than thelever portion 50 causing no obstacle in measurements (for example on thesupport portion 54).

Here silicon nitride having greater silicon content is used as the probeportion 49 and lever portion 50 for the reason as follows. While, alsoin this embodiment, an elemental ratio between silicon (Si) and nitrogen(N) of the silicon nitride film in the range of 0.75<Si/N≦1.3 is used,such range is an optimal elemental ratio range for the structure of athin film such as cantilever. Particularly regarding stress, if theelemental ratio is Si/N≦0.75, an intense tensile stress of 1,000 MPa orabove results. Because of this, warping at the lever portion occurs orthe tip of the probe portion is cracked due to stress. In the range ofSi/N>1.3, on the other hand, since Si is polycrystallized and causes aprecipitation, the surface coarseness is worsened and it becomesdisadvantageous for example for a cantilever in which a smooth leverportion surface or probe portion surface is desired. Also in asubsequent silicon etching process, an etchant may permeate from thepolycrystallized silicon portion to result an abnormal etching. Toprevent such abnormal etching, the above described elemental ratio rangeis used.

By such fabricating method, the cantilever made of silicon nitridehaving a radius of curvature at the tip of the probe portion sharpenedto 20 nm or less and at the same time having a high aspect ratio can bereadily fabricated without using a high precision apparatus which isexpensive.

Further, since the probe portion having the sharpened terminal endportion can be fabricated in a well regulated manner and at high yield,costs can also be reduced. Furthermore, batch processing of a pluralityof cantilevers at wafer level becomes possible.

In particular, unlike the conventional method in which a resist mask isprepared and an underetching is effected while regulating the etchantand time, the length of the sharpened portion of the probe terminal endportion in the fabricating method according to the present embodiment isnot restricted by the limitation due to the permeation of etchant underthe mask so that the sharpened portion (terminal end portion) havinggreater length can be made. Further, in the fabricating method accordingto the present embodiment, it is adequate that only the oxidized portionformed on the silicon nitride film surface be entirely etched away byfluoric acid. It is thereby also possible to secure far greaterprocessing margin for example in control of the temperature andconcentration of etchant and control of etching time as compared to anisotropic wet etching of which control is generally considered to bedifficult.

In the case where a further improvement in the aspect ratio of the probeportion or further sharpening of the tip of the terminal end portionthereof is desired, the above described process can be repeated for aplurality of times to additionally promote the sharpening.

Further, of the cantilever having the plate-like probe portion asdescribed in the first embodiment, i.e., bird's-beak probe portion, therigidity of the probe portion is lowered when the length of the probeportion is increased. In performing measurements by attaching it to ascanning probe microscopy, therefore, the probe portion is easilydistorted and it becomes difficult when acted upon by a force exertedfrom a sample to accurately ascertain surface irregularities of thesample. Of the cantilever having the triangular pyramidal probe portiondescribed in the present embodiment, however, the mechanical rigidity ofthe probe portion is high and the surface irregularities of a sample canbe accurately ascertained even if the probe length is made longer.

It should be noted that the present embodiment has been shown as thatusing RIE in etching the silicon nitride film in the step shown in FIG.8F. It is however not limited to the use of RIE and other dry etcherssuch as ICP-RIE or an wet etching for example of hot phosphoric acid canalso be used. This is because the surface oxidation is not affected bythe configuration of the silicon nitride film before the oxidation step.

The fabricating method according to the above second embodiment issummarized as follows. Since uniform probe portions can be formed allover a wafer by a combination of simple processes, namely,low-temperature thermal oxidation and wet etching by fluoric acid, it ispossible to readily fabricate a cantilever of which the terminal endportion can be sharpened in a well regulated manner and which has apyramidal or conic probe portion having a high aspect ratio. Further,since the probe portions of a large number of cantilevers to be formedon a plurality of pieces of wafer can be formed by sharpening them atonce, the yield thereof is higher and costs can be reduced.

Further, the present embodiment has been shown as that using atriangular pyramidal probe portion as the probe portion because of thefeasibility of readily and dependably forming a projection terminatingat a point. The probe portion in the form of a pyramid or cone accordingto the present embodiment, however, is not limited to a triangularpyramidal form and naturally also applicable to a probe portion in theform of a circular cone. In the case of the circular-conic probeportion, it suffices to apply an overcoating of silicon nitride over asilicon projection in the form of a circular cone. With thecircular-conic probe portion, the mechanical rigidity becomes higher andthe terminal end portion of the probe portion becomes bilaterallysymmetrical, and the tip thereof is further sharpened so that stablemeasured images can be obtained without being influenced by the scanningdirection of cantilever in SPM measurements. Further, the cantilever canbe achieved as having a probe portion of which the tip is dependablysharpened and which has a sufficient length even in the case ofmeasuring a smaple having greater surface irregularities.

1. An SPM cantilever comprising a support portion, a lever portionextended from the support portion and a probe portion formed at a freeend of the lever portion, wherein said probe portion is generallypyramidal or conic and the pyramidal or conic probe portion has anadditionally sharpened terminal end portion.
 2. The SPM cantileveraccording to claim 1, wherein said probe portion is generally in theform of a triangular pyramid.
 3. The SPM cantilever according to claim1, wherein said probe portion is generally in the form of a circularcone.
 4. The SPM cantilever according to claim 1, wherein said probeportion is formed of silicon nitride.
 5. The SPM cantilever according toclaim 2, wherein said probe portion is formed of silicon nitride.
 6. TheSPM cantilever according to claim 3, wherein said probe portion isformed of silicon nitride.